WO2011027911A1 - Élément photosensible électrophotographique, cartouche de traitement et appareil électrophotographique - Google Patents

Élément photosensible électrophotographique, cartouche de traitement et appareil électrophotographique Download PDF

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Publication number
WO2011027911A1
WO2011027911A1 PCT/JP2010/065569 JP2010065569W WO2011027911A1 WO 2011027911 A1 WO2011027911 A1 WO 2011027911A1 JP 2010065569 W JP2010065569 W JP 2010065569W WO 2011027911 A1 WO2011027911 A1 WO 2011027911A1
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WO
WIPO (PCT)
Prior art keywords
conductive layer
electrophotographic photosensitive
photosensitive member
tin oxide
particles
Prior art date
Application number
PCT/JP2010/065569
Other languages
English (en)
Inventor
Atsushi Fujii
Haruyuki Tsuji
Hideaki Matsuoka
Kazuhisa Shida
Nobuhiro Nakamura
Original Assignee
Canon Kabushiki Kaisha
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Canon Kabushiki Kaisha filed Critical Canon Kabushiki Kaisha
Priority to RU2012112931/28A priority Critical patent/RU2507554C2/ru
Priority to KR1020127007842A priority patent/KR101400650B1/ko
Priority to CN2010800389861A priority patent/CN102483592B/zh
Priority to US13/384,852 priority patent/US9256145B2/en
Priority to EP10813856.1A priority patent/EP2443518B1/fr
Priority to BR112012004861A priority patent/BR112012004861A2/pt
Publication of WO2011027911A1 publication Critical patent/WO2011027911A1/fr
Priority to US14/095,955 priority patent/US10073362B2/en

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Classifications

    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/08—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/043—Photoconductive layers characterised by having two or more layers or characterised by their composite structure
    • G03G5/047—Photoconductive layers characterised by having two or more layers or characterised by their composite structure characterised by the charge-generation layers or charge transport layers
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/10—Bases for charge-receiving or other layers
    • G03G5/104—Bases for charge-receiving or other layers comprising inorganic material other than metals, e.g. salts, oxides, carbon
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/14—Inert intermediate or cover layers for charge-receiving layers
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/14—Inert intermediate or cover layers for charge-receiving layers
    • G03G5/142—Inert intermediate layers
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/14—Inert intermediate or cover layers for charge-receiving layers
    • G03G5/142—Inert intermediate layers
    • G03G5/144—Inert intermediate layers comprising inorganic material

Definitions

  • This invention relates to an electrophotographic
  • photosensitive members organic electrophotographic photosensitive members
  • the electrophotographic photosensitive member is
  • a layer containing metal oxide particles is known as the layer formed for the purpose of covering any defects of the surface of the support.
  • the layer containing metal oxide particles commonly has a higher electrical conductivity than a layer not containing any metal oxide particles (e.g., 5.0*10 8 to 1.0*10 13 ⁇ -cm as volume resistivity).
  • conductivity (hereinafter "conductive layer) makes the support surface have a great tolerance for its defects. As the results, this makes the support have a vastly great tolerance for its use, and hence brings an
  • the electrophotographic photosensitive member can be improved in productivity.
  • Patent Literature 1 discloses a technique in which tin oxide particles doped with phosphorus are used in a layer formed between the support . and the photosensitive layer.
  • Patent Literature 2 also discloses a technique in which tin oxide particles doped with tungsten are used in a protective layer formed on the photosensitive layer.
  • Patent Literature 3 still also discloses a technique in which titanium oxide particles coated with oxygen deficient tin oxide are used in a conductive layer formed between the support and the photosensitive layer.
  • Patent Literatures 4 and 5 still also disclose a technique in which barium sulfate particles coated with tin oxide are used in a layer formed between the support and the photosensitive layer.
  • Literature 6 still also discloses a technique in which titanium oxide particles coated with indium oxide doped with tin (indium oxide-tin oxide) are used in a layer formed between the support and the photosensitive layer.
  • charging lines comes to tend to occur in reproduced images when images are formed in a low- temperature and low-humidity environment by using an ⁇ electrophotographic photosensitive ; member employing as the conductive layer any layer containing such metal oxide particles as the above.
  • the charging lines refer to line-like faulty images appearing in the direction perpendicular to the peripheral direction of the surface of the electrophotographic photosensitive member, which are caused by a lowering of uniformity in surface potential (i.e., non-uniform charging) of an electrophotographic photosensitive member when the surface of the ' electrophotographic photosensitive . , member is electrostatically charged, and tend to remarkably appear when halftone images are reproduced.
  • An object of the present invention is to provide an electrophotographic photosensitive' member that can not easily cause such charging lines even where it is an electrophotographic photosensitive member employing as the conductive layer the layer containing metal oxide particles, and a process cartridge and an
  • electrophotographic apparatus which have such an electrophotographic photosensitive member.
  • the present invention is an electrophotographic photosensitive member which comprises a support, a conductive layer formed on the support, and a
  • the conductive layer contains a binding material, and titanium oxide particles coated with tin oxide doped with phosphorus or tungsten.
  • the present invention is also a process cartridge
  • electrophotographic photosensitive member and at least one means selected from the group consisting of a charging means, a developing means, a transfer means and a cleaning means, and is detachably
  • electrophotographic apparatus which comprises, the above electrophotographic photosensitive member, and a charging means, an exposure means, a developing means and a transfer means.
  • the present invention can provide an electrophotographic photosensitive member that can not easily cause charging lines even where it is an
  • electrophotographic photosensitive member employing as the conductive layer the layer containing metal oxide particles, and a process cartridge and an
  • electrophotographic apparatus which have such an electrophotographic photosensitive member.
  • Fig. 1 is a view showing schematically an
  • Fig. 2 is a view (plan view) to illustrate how to measure the volume resistivity of a conductive layer.
  • Fig. 3 is a view (sectional view), to illustrate how to measure the volume resistivity of a conductive layer .
  • present invention is an electrophotographic
  • the photosensitive member having a support, a conductive layer formed on the support, and a photosensitive layer formed on the conductive layer.
  • the photosensitive layer may be a single-layer type photosensitive layer which contains a charge-generating material and a charge-transporting material in a- single layer, or may be a multi-layer type photosensitive layer . formed in layers of a charge generation layer which contains a charge-generating material and a charge transport layer which contains a charge-transporting material.
  • subbing layer may also optionally be provided between the conductive layer and the photosensitive layer.
  • the support it may preferably be one having
  • a metallic support which is made of a metal, formed of a metal such as aluminum, an aluminum alloy or stainless steel.
  • a metallic support which is made of a metal, formed of a metal such as aluminum, an aluminum alloy or stainless steel.
  • aluminum or an aluminum alloy is used, usable are an aluminum pipe produced by a production process having the step of extrusion and the step of drawing, and an aluminum pipe produced by a production process having the step of extrusion and the step of ironing.
  • Such aluminum pipes can achieve a good dimensional precision and surface smoothness without requiring any surface cutting and besides are advantageous in view of cost as well.
  • a conductive layer which contains a binding material and titanium oxide (Ti0 2 ) particles coa-ted with tin oxide (Sn0 2 ) doped with phosphorus (P) or tungsten (W), is formed on the support.
  • the titanium oxide (Ti0 2 ) particles coated with tin oxide (Sn0 2 ) doped with phosphorus (P) or tungsten (W) are hereinafter also termed "phosphorus- or tungsten- doped tin oxide coated titanium oxide particles".
  • the conductive layer may preferably have a volume
  • the conductive layer preferably 5.0*10 12 ⁇ -cm or less. If a layer having too high volume resistivity is provided on the support as the layer for covering any defects of the surface of ⁇ the support, the flow of electric charges tends to stagnate therein to tend to increase in residual potential. Also, from the viewpoint of keeping the charging lines from occurring, too, it is preferable for the conductive layer to have a low volume
  • the conductive layer may on the other hand preferably have a volume resistivity of 1.0*10 8 ⁇ -cm or more, and much preferably 5.0 10 8 ⁇ -cm or more. If the conductive layer has too low volume resistivity, the electric charges flowing through the conductive layer may be so large in quantity that dots and/or fog due to the injection of electric charges from the support into the photosensitive layer may tend to occur in reproduced images when images are repeatedly formed in a high-temperature and high-humidity environment.
  • the volume resistivity of the conductive layer is.
  • a tape 203 made of copper (Type No.1181, available from Sumitomo 3M Limited) is stuck to the surface of a conductive layer 202 to make it serve as an electrode on the surface side of the conductive layer 202.
  • a support 201 is also made to serve as an electrode on the back side of the
  • a power source 206 and a current measuring instrument 207 are respectively set up; the former for applying voltage across the copper tape 203 and the support 201 and the latter for measuring
  • a copper wire 204 is put on the copper tape 203, and then a tape 205 made of copper like the copper tape 203 is stuck from above the copper wire 204 to the copper tape 203 so that the copper wire 204 may not protrude from the copper tape 203, to fasten the copper wire 204 to the copper tape 203.
  • a tape 205 made of copper like the copper tape 203 is stuck from above the copper wire 204 to the copper tape 203 so that the copper wire 204 may not protrude from the copper tape 203, to fasten the copper wire 204 to the copper tape 203.
  • d thickness of the conductive layer 202
  • S area of the electrode (copper tape 203) on the surface side of the conductive layer 202
  • p volume resistivity p ( ⁇ -cm) of the conductive layer 202.
  • the level of electric current of extremely as small as 1 ⁇ 10 ⁇ 6 A or less is measured, and hence it is preferable to make the measurement by using as the current measuring instrument 207 an instrument that can measure an extremely small electric current.
  • an instrument may include, e.g., a pA meter (trade name: 4140B) manufactured by Yokogawa Hewlett-Packard Company.
  • the volume resistivity of the conductive layer shows the like value in either of measurement made in the state only the conductive layer has been formed on the support or measurement made in the state the respective layers (photosensitive layer and . so forth) on the conductive layer have been stripped off the electrophotographic photosensitive member so as to leave only the conductive layer on the support.
  • Ti0 2 titanium oxide
  • W tungsten
  • Sn0 2 tungsten
  • tungsten (W) -doped tin oxide (Sn0 2 ) particles particles (particles composed of only phosphorus ( P) - or tungsten ( ) -doped tin oxide (Sn0 2 ) ) are used as the metal oxide particles, the metal oxide particles in the conductive layer coating fluid tend to have a large particle diameter, so that protruding spotty defects may occur on the surface of the conductive layer or the conductive layer coating fluid may become low stable.
  • the titanium oxide (Ti0 2 ) particles are used as the core particles, because their use is highly effective in keeping the charging lines from occurring, and further because such particles have so low transparency as to easily cover any defects on the surface of the support. On the other hand, if, e.g., barium sulfate particles are used as the core particles, this makes it difficult to keep the charging lines from occurring. In addition, because of their high transparency as metal oxide particles, this may additionally require any material for covering the defects on the surface of the support.
  • titanium oxide coated titanium oxide particles are more highly effective in keeping the charging lines from occurring than titanium oxide (Ti0 2 ) particles coated with oxygen deficient tin oxide (Sn0 2 ) - Further, compared with the titanium oxide (Ti0 2 ) particles coated with oxygen deficient tin oxide (Sn0 2 ), the former particles are less causative of any increase in volume resistivity in a low-humidity environment and any decrease in- volume resistivity in a high-humidity environment, an also have superior environmental stability.
  • tungsten (W) -doped tin oxide (Sn0 2 ) coated titanium oxide (Ti0 2 ) ⁇ particles is also disclosed in Japanese Patent Applications Laid-open No. H06-207118 and No. 2004-349167.
  • the conductive layer In order for the conductive layer to keep its volume resistivity within the above range, it is preferable to use, in preparing the conductive layer coating fluid used in forming the conductive layer, phosphorus- or tungsten-doped tin oxide coated titanium oxide
  • the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles may more preferably have a powder resistivity of from 1.0x10° ⁇ -cm or more to 1.0*10 5 ⁇ -cm or less, much preferably from 1.0*10° ⁇ -cm or more to 1.0*10 3 ⁇ -cm or less, and much more preferably from 1.0x10° ⁇ -cm or more to 1.0*10 2 ⁇ -cm or less. If the
  • phosphorus- or tungsten-doped tin oxide coated titanium oxide particles have too high powder resistivity, it is difficult to control the conductive layer to have the volume resistivity of ⁇ . ⁇ ⁇ ⁇ 13 ⁇ cm or less, or 5.0*10 12 ⁇ -cm or less. If on the other hand the phosphorus- or tungsten-doped tin oxide coated titanium oxide
  • the tin oxide (Sn0 2 .) may preferably be in a proportion (coverage) of from 10% by mass to 60% by mass, and much preferably from 15% by mass to 55% by mass.
  • a tin raw material necessary to form the tin oxide (Sn0 2 ) must be compounded when the
  • phosphorus- or tungsten-doped tin oxide coated titanium oxide particles are produced.
  • such phosphorus- or tungsten-doped tin oxide coated titanium oxide particles are produced.
  • Sn0 2 is defined to be a value calculated from the mass of tin oxide (Sn0 2 ) that is based on the total mass of the tin oxide (Sn0 2 ) and the titanium oxide (Ti0 2 ), without taking account of the mass of the phosphorus ( P) or tungsten (W) with which the tin oxide (Sn0 2 ) is doped. Any too small coverage of the tin oxide (Sn0 2 ) makes it difficult to control the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles to have the powder resistivity of ⁇ . ⁇ ⁇ ⁇ 6 ⁇ -cm or less. Any too large coverage thereof tends to make the titanium oxide (Ti0 2 ) particles non-uniformly coated with tin oxide (Sn0 2 ) , and also tends to result in a high cost.
  • any too small dope level of the tin oxide (Sn0 2 ) is doped may preferably be in an amount (dope level) of from 0.1% by mass to 10% by mass based on the mass of the tin oxide (Sn0 2 ) to be doped (the mass not inclusive of that of the phosphorus ( P) or tungsten (W) ) . Any too small dope level of the tin oxide (Sn0 2 ) is doped (hereinafter also phosphorus or tungsten "doped to tin oxide”) may preferably be in an amount (dope level) of from 0.1% by mass to 10% by mass based on the mass of the tin oxide (Sn0 2 ) to be doped (the mass not inclusive of that of the phosphorus ( P) or tungsten (W) ) . Any too small dope level of the tin oxide (Sn0 2 ) is doped (hereinafter also phosphorus or tungsten "doped to tin oxide”) may
  • the tin oxide (Sn0 2 ) is doped makes the tin oxide (Sn0 2 ) have a low crystallizability to make it difficult to control the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles to have the powder resistivity of from 1.0x10° ⁇ -cm or more to ⁇ . ⁇ ⁇ ⁇ 6 ⁇ -cm or less.
  • phosphorus (P) or tungsten (W) can make particles have a low powder resistivity.
  • Mitsubishi Chemical Corporation (trade name: . LORESTA GP) is used as a measuring instrument.
  • the measurement object phosphorus- or tungsten-doped tin oxide coated titanium oxide particles are compacted at a pressure of 500 kg/cm 2 to prepare a pellet-shaped measuring sample.
  • the powder resistivity is measured at an applied
  • photosensitive member to have a dielectric loss tan5 at frequency ⁇ . ⁇ ⁇ ⁇ 3 Hz, of from 5 ⁇ 10 ⁇ 3 or more to 2*10 "2 or less .
  • orientation polarization is a phenomenon where displacement of electric charges takes place in a dielectric placed into an electric field.
  • One type of this dielectric polarization is the orientation polarization that is caused by changes in direction of dipole moments in any molecules constituting that dielectric.
  • the surface of the electrophotographic photosensitive member is provided with electric charges on its
  • an electric field is produced by these electric charges (hereinafter called “external electric field”) .
  • external electric field dipole moments inside the electrophotographic photosensitive member gradually come into polarization (orientation polarization) .
  • the sum of vectors of the dipole moments having thus polarized comes to the electric field that has been produced inside the electrophotographic photosensitive member as a result of the polarization (hereinafter called “internal electric field”) .
  • the internal electric field With lapse of time, the polarization progresses, and the internal electric field becomes larger .
  • electrophotographic photosensitive member may be found by adding the external electric field and the ⁇ internal electric field, thus it is considered that the total sum of electric field intensities decreases gradually with progress of the polarization.
  • electrophotographic photosensitive member substantially does not change, and hence the potential difference and the electric field are considered to stand a
  • the dielectric loss tan6 is used in the present invention.
  • the dielectric loss tan5 is the heat loss of energy that is based on the progress of orientation polarization in an alternating-current electric field, and serves as an index of time
  • electrophotographic photosensitive member that is caused by the progress of orientation polarization is influenced by how far the orientation polarization progresses during the time (usually about ⁇ . ⁇ ⁇ ⁇ -3 second) starting when the surface of the
  • electrophotographic photosensitive member is provided with electric charges on its charging region upstream side and ending when the surface of the
  • electrophotographic photosensitive member is provided with electric charges on its charging region downstream side. If the orientation polarization is not completed during this time, the orientation polarization may inevitably progress before the surface of the
  • electrophotographic photosensitive member is provided with electric charges on its charging region downstream side, and hence the electrophotographic photosensitive member decreases in its surface potential, as so considered.
  • measuring the dielectric loss tan5 enables prediction of the charging lines, and extent thereof, caused by the decrease in surface potential of electrophotographic photosensitive member that is attended by the progress of orientation
  • electrophotographic photosensitive member is described below .
  • the electrophotographic photosensitive member is cut along its surface into small pieces (10 mm ⁇ 10 mm each) .
  • the electrophotographic photosensitive member is cylindrical, pieces with curved surfaces are each so stretched with a vise or the like as to become planar.
  • gold (an electrode) 600 nm in thickness is vacuum-deposited to prepare a measuring sample.
  • it is vacuum-deposited by means of a sputtering apparatus ⁇ (trade name: SC-707 QUICK COATER) manufactured by Sanyu Denshi Co., Ltd.
  • SC-707 QUICK COATER trade name: SC-707 QUICK COATER
  • photosensitive member measuring sample is measured in the like environment under conditions of a frequency of ⁇ . ⁇ ⁇ ⁇ 3 Hz and an applied voltage of 100 mV.
  • the dielectric loss tan5 is measured with an impedance analyzer (trade name: Frequency
  • he measuring sample may also be prepared by forming each layer like that of the measurement object
  • the photosensitive member having the conductive layer have a correlation, where the dielectric loss tan5 of the electrophotographic photosensitive member having the conductive layer shows a tendency to increase with an increase in the volume resistivity of the conductive layer .
  • electrophotographic photosensitive member having the conductive layer containing the phosphorus- .
  • photosensitive member having a conductive . layer
  • the use of the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles makes it easy to keep charging lines from occurring while keeping dots and/or fog from occurring.
  • the conductive layer may be formed by coating a
  • conductive layer coating fluid obtained by dispersing the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles in a solvent together with a binding material, and drying and/or curing the wet coating formed.
  • a method for dispersion it may include, e.g., a method making use of a paint shaker, a sand mill, a ball mill or a liquid impact type highspeed dispersion machine.
  • conductive layer it may include, e.g., phenol resin, polyurethane resin, polyamide resin, polyimide resin, polyamide-imide resin, polyvinyl acetal resin, epoxy resin, acrylic resin, melamine resin, and polyester resin. Any of these may be used alone or in
  • hardening resins are preferred, and heat-hardening resins (thermosetting resins) are much preferred.
  • thermosetting resins thermosetting phenol resins and thermosetting ' polyurethane resins are preferred. Where such a thermosetting resin is used as the binding material for the conductive layer, the binding material to be contained in the conductive layer coating fluid serves as a monomer, and/or an oligomer, of thermosetting resin.
  • coating fluid may include, e.g., alcohols such as methanol, ethanol and isopropanol; ketones such as ' acetone, methyl ethyl ketone and cyclohexanone; ethers such as tetrahydrofuran, dioxane, ethylene glycol monomethyl ether and propylene glycol monomethyl ether; esters such as methyl acetate and ethyl acetate; and ⁇ aromatic hydrocarbons such as toluene and xylene.
  • alcohols such as methanol, ethanol and isopropanol
  • ketones such as ' acetone, methyl ethyl ketone and cyclohexanone
  • ethers such as tetrahydrofuran, dioxane, ethylene glycol monomethyl ether and propylene glycol monomethyl ether
  • esters such as methyl acetate and ethyl acetate
  • ⁇ aromatic hydrocarbons such
  • the phosphorus- or tungsten- doped tin oxide coated titanium oxide particles (P) and binding material (B) in the conductive layer coating fluid may preferably be in a mass ratio (P/B) of from 1.0/1.0 or more to 3.5/1.0 or less. Any too smaller quantity of the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles than the binding material may make it difficult to control the
  • any too larger quantity of the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles than the binding material may make it
  • the volume resistivity of 1.0*10 8 ⁇ -cm or more or 5.0 ⁇ 10 8 ⁇ -cm or more. Any too larger quantity of the
  • phosphorus- or tungsten-doped tin oxide coated titanium oxide particles than the binding material may also make it difficult to bind the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles, to tend to cause cracks in the conductive layer.
  • the conductive layer may preferably have a layer thickness of from 10 ⁇ or more to 40 ⁇ or less, and much preferably from 15 m or more to 35 ⁇ or less.
  • the layer thickness of each layer, inclusive of the conductive layer, of the electrophotographic photosensitive member is measured with FISCHERSCOPE Multi Measurement System (nuns), available from Fisher Instruments Co.
  • titanium oxide particles in the conductive layer coating fluid may preferably have an average particle diameter of from 0.10 ⁇ or more to 0.60 ⁇ or less, and much preferably from 0.15 ⁇ or more to 0.45 ⁇ or less. If the phosphorus- or tungsten-doped tin oxide coated titanium oxide particles have too small average particle diameter, such oxide particles may come to agglomerate again after the conductive layer coating fluid has been prepared, to make the conductive layer coating fluid low stable or cause cracks in the
  • the surface of the conductive layer may come so rough as to tend to cause local injection of electric charges therefrom into the photosensitive layer, so that dots may conspicuously appear in white background areas of reproduced images.
  • particles in the conductive layer coating fluid may be measured by liquid-phase sedimentation in the following way.
  • the conductive layer coating fluid is so diluted with the solvent used in preparing the same, as to have a transmittance between 0.8 and 1.0.
  • centrifugal automatic particle size distribution measuring instrument a centrifugal automatic particle size distribution measuring instrument (trade name: CAPA700) manufactured by Horiba, Ltd. is used to make measurement under conditions of a number of revolutions of 3,000 rpm.
  • a surface roughness providing material for roughening the surface of the conductive layer may also be added to the conductive layer coating fluid.
  • a surface roughness providing material may preferably be resin particles having an average particle . diameter of from 1 ⁇ or more to 5 ⁇ or less (preferably 3 ⁇ or less) .
  • Such resin particles may include, e.g.,
  • particles of hardening rubbers and of hardening resins such as polyurethane, epoxy resin, alkyd resin, phenol resin, polyester, silicone resin and acryl-melamine resin. Of these, particles of silicone resin are preferred as being less agglomerative .
  • the specific gravity of resin particles (which is 0.5 to 2). is smaller than the specific gravity of the phosphorus- or tungsten-doped tin oxide coated titanium oxide
  • the conductive layer has a tendency to increase in volume resistivity with an increase in content of the surface roughness providing material in the conductive layer.
  • the content of the surface roughness providing material in the conductive layer coating fluid may preferably be from 1 to 80% by mass, and much
  • a leveling agent may also be added in order to enhance the surface properties of the conductive layer.
  • Pigment particles may also be added to the conductive layer coating fluid in order to improve covering properties of the
  • a subbing layer also called a barrier layer or an intermediate layer having electrical barrier
  • properties may be provided in order to block the injection of electric charges from the conductive layer into the photosensitive layer.
  • the subbing layer may be formed by coating on the
  • the resin (binder resin) used for the subbing layer may include, e.g., water-soluble resins such as polyvinyl alcohol, polyvinyl methyl ether, polyacrylic acids, methyl cellulose, ethyl cellulose, polyglutamic acid, casein, and starch; and polyamide, polyimide,
  • thermoplastic resins are preferred.
  • thermoplastic resins a thermoplastic resin selected from the thermoplastic resins.
  • thermoplastic polyamide is preferred.
  • polyamide copolymer nylon or the like is preferred.
  • he subbing layer may preferably have a layer thickness of from 0.1 ⁇ or more to 2 ⁇ i or less.
  • the subbing layer may also be incorporated with an electron-transporting material.
  • the photosensitive layer is formed on the conductive . layer (a subbing layer) .
  • photosensitive layer may include, e.g., azo pigments such as monoazo, disazo and trisazo, phthalocyanine pigments such as metal phthalocyanines and metal-free phthalocyanine, indigo pigments such as indigo and thioindigo, perylene pigments such as perylene acid anhydrides and perylene acid imides, polycyclic quinone pigments such as anthraquinone and pyrenequinone, squarilium dyes, pyrylium salts and ⁇ thiapyrylium . salts , triphenylmethane dyes, quinacridone pigments, azulenium salt pigments, cyanine dyes, xanthene dyes,
  • azo pigments such as monoazo, disazo and trisazo
  • phthalocyanine pigments such as metal phthalocyanines and metal-free phthalocyanine
  • indigo pigments such as indigo and thioindigo
  • quinoneimine dyes and styryl dyes.
  • metal phthalocyanines such as oxytitanium phthalocyanine, hydroxygallium phthalocyanine and chlorogallium phthalocyanine.
  • the charge generation layer may be formed by coating a charge generation layer coating fluid obtained by dispersing the charge generating material in a solvent together with a binder resin, and drying the wet coating formed.
  • a method for dispersion a method is available which makes use of a homogenizer, ultrasonic waves, a ball mill, a sand mill, an attritor or a roll mill.
  • layer may include, e.g., polycarbonate, polyester, polyarylate, butyral resin, polystyrene, polyvinyl acetal, diallyl phthalate resin, acrylic resin,
  • methacrylic resin vinyl acetate resin, phenol resin, silicone resin, polysulfone, styrene-butadiene
  • copolymer alkyd resin, epoxy resin, urea resin, and vinyl chloride-vinyl acetate copolymer. Any of these may be used alone or in the form. of a mixture or copolymer of two or more types.
  • the charge ⁇ generating material and- the binder resin may preferably be in a proportion (charge generating material : binder resin) ranging from 10:1 to 1:10 (mass ratio), much preferably from 5:1 to 1:1 (mass ratio), and much more preferably from 3:1 to 1:1 (mass ratio) .
  • coating fluid may include, e.g., alcohols, sulfoxides, ketones, ethers, esters, aliphatic halogenated
  • the charge generation layer may preferably have a layer thickness of 5 ⁇ or less, and much preferably from 0.1 ⁇ or more to 2 ⁇ or less.
  • antioxidant an ultraviolet absorber, a plasticizer and so forth which may be of various types may also be used.
  • An electron transport material (an electron accepting material such as an acceptor) may also be incorporated in the charge generation layer in order to make the flow of electric charges not stagnate in the charge generation layer.
  • photosensitive layer may include, e.g., triarylamine compounds, hydrazone compounds, styryl compounds, stilbene compounds, pyrazoline compounds, oxazole compounds, thiazole compounds, and triarylmethane compounds .
  • the charge transport layer may be formed by coating a charge transport layer coating fluid obtained by dissolving the charge
  • layer may include, e.g., acrylic resin, styrene resin, polyester, polycarbonate, polyarylate, polysulfone, polyphenylene oxide, epoxy resin, polyurethane, alkyd resin and unsaturated resins. Any of these may be Used alone or in the form of a mixture or copolymer of two or more types.
  • the charge transporting material and the binder resin may preferably be in a proportion (charge transporting material : binder resin) ranging from 2:1 to 1:2 (mass ratio) .
  • the solvent used in the charge transport layer coating fluid may include, e.g., ketones such as acetone and methyl ethyl ketone, esters such as methyl acetate and ethyl acetate, ethers such as dimethoxymethane and dimethoxyethane, aromatic hydrocarbons such as toluene and xylene, and hydrocarbons substituted with a halogen atom, such as chlorobenzene, chloroform and carbon tetrachloride .
  • ketones such as acetone and methyl ethyl ketone
  • esters such as methyl acetate and ethyl acetate
  • ethers such as dimethoxymethane and dimethoxyethane
  • aromatic hydrocarbons such as toluene and xylene
  • hydrocarbons substituted with a halogen atom such as chlorobenzene, chloroform and carbon tetrachloride .
  • the charge transport layer may preferably have a layer thickness of from 3 ⁇ or more to 40 ⁇ or less, and much preferably from 5 ⁇ or more to 30 ⁇ or less, from the viewpoint of charging uniformity and image reproducibility.
  • ultraviolet absorber a plasticizer and so forth may also optionally be added.
  • the single-layer type photosensitive layer may be formed by
  • coating fluid containing a charge generating material, a charge transporting material, a binder resin and a solvent, and drying the wet coating formed.
  • charge transporting material As these charge generating material, charge transporting
  • a protective layer may also be provided on the photosensitive layer.
  • the protective layer may be formed by coating a protective layer coating fluid containing a resin (binder resin) , and drying and/or curing the wet coating formed.
  • the binder resin used to form the protective layer may include, e.g., phenol resin, acrylic resin, polystyrene, polyester, polycarbonate, polyarylate, polysulfone, polyphenylene oxide, epoxy resin, polyurethane, alkyd resin, siloxane resin and unsaturated resins. Any of these may be used alone or in the form of a mixture or copolymer of two or more types.
  • the protective layer may preferably have a layer thickness of from 0.5 ⁇ or more to 10 ⁇ or less, and much preferably from 1 ⁇ or more to 8 ⁇ or less.
  • coating fluids for the above respective layers are coated, usable are coating methods as exemplified by dip coating (dipping) , spray coating, spinner coating, roller coating, Mayer bar coating and blade coating.
  • FIG. 1 schematically shows an example of the
  • reference numeral 1 denotes a drum-shaped electrophotographic photosensitive member, which is rotatingly driven around an axis 2 in the direction of an arrow at a stated peripheral speed.
  • photosensitive member 1 rotatingly driven is uniformly electrostatically charged to a positive or negative, stated potential through a charging means (primary charging means; ⁇ e.g. , a charging roller) 3.
  • the electrophotographic photosensitive member thus charged is then exposed to exposure light (imagewise exposure light) 4 emitted from an exposure means (an imagewise exposure means; not shown) for slit exposure, laser beam scanning exposure or the like.
  • exposure light imagewise exposure light
  • Voltage to be applied to the charging means 3 may be only direct-current voltage or may be direct-current voltage on which alternating- current voltage is kept superimposed.
  • the photosensitive member 1 are developed with a toner of a developing means 5 to form toner images. Then, the toner- images thus formed and held on the peripheral surface of the electrophotographic photosensitive member 1 are transferred to a transfer material (such as paper) P by applying a transfer bias from a transfer means (such as a transfer roller) 6.
  • the transfer material P is fed through a transfer material feed means (not shown) to come to the part (contact zone) between the electrophotographic photosensitive member 1 and the transfer means 6 in the manner synchronized with the rotation of the electrophotographic
  • the transfer material P to which the toner images have been transferred is separated from the peripheral surface of the electrophotographic photosensitive member 1 and is led into a fixing ' means 8, where the toner images are fixed, and is then put out of the apparatus as an image-formed material (a print or copy) .
  • photosensitive member 1 from which toner images have been transferred is brought to removal of the toner remaining after the transfer, through a cleaning means (such as a cleaning blade) 7. It is further subjected to charge elimination by pre-exposure light 11 emitted from a pre-exposure means (not shown) , and thereafter . repeatedly used for the formation of images.
  • a cleaning means such as a cleaning blade
  • the pre-exposure is not necessarily required where the charging means is a contact charging means .
  • the apparatus may be constituted of a combination of
  • a conductive substrate constituted of, e.g., a conductive substrate and one or more cover layers formed on the conductive substrate. At least one layer of the cover layers is also provided with conductivity.
  • it may be constituted of a conductive substrate, a conductive elastic layer formed on the conductive substrate and a surface layer formed on the conductive elastic layer.
  • the charging roller may preferably have a surface of
  • Rzjis roughness of the surface of the charging roller is measured with a surface profile analyzer (trade name: SE-3400) manufactured by Kosaka Laboratory Ltd. More specifically, using this surface profile analyzer, the Rzjis is measured at arbitrary six spots on the surface of the charging roller, and an arithmetic mean value of values found at the six spots is taken as the ten-point average roughness (Rzjis) of the surface of the charging roller.
  • the toner and its external additives tend to adhere to the surface of the charging roller, so that faulty images caused by staining of the surface of the charging roller may occur.
  • the surface of the charging roller is controlled to have the ten-point average roughness (Rzjis) of 5.0 ⁇ or less, the difference in discharge level that is due to difference in height of surface profile of the surface of the charging roller can be kept small. Thus, this can keep any faulty images such as dots from occurring because of any faulty charging caused by the profile of the surface of the charging roller.
  • part(s) refers to “part(s) by mass”. Titanium oxide (Ti0 2 ) particles (core particles) in the phosphorus- or tungsten-doped tin oxide coated titanium oxide
  • particles as used in the following working examples are all those having a BET value of 6.6 m 2 /g..
  • silicone resin particles (trade name: TOSPEARL 120; available from GE Toshiba Silicones; average particle diameter: 2 ⁇ ) as a surface roughness providing material
  • silicone oil (trade name: SH28PA; available from Dow Corning Toray Silicone Co., Ltd.) as a leveling agent
  • 6 parts of methanol and 6 parts of l-methoxy-2-propanol were added to the fluid dispersion, followed by
  • the phosphorus ( P) -doped tin oxide (SnC>2 ) coated titanium oxide (Ti0 2 ) particles in the conductive layer coating fluid 1 had an average particle diameter of 0.35 ⁇ .
  • Conductive layer coating fluids 2 to 20 were prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that the metal oxide particles (phosphorus- or tungsten-doped tin oxide coated titanium oxide particles) used therein in preparing the conductive layer coating fluid were respectively changed as shown in Table 1.
  • the average particle diameters of the metal oxide particles were respectively changed as shown in Table 1.
  • a conductive layer coating fluid CI was prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that 204 parts of the metal oxide particles, phosphorus ( P) -doped tin oxide (Sn0 2 ) coated titanium oxide (Ti0 2 ) particles, used therein in preparing the conductive layer coating fluid were changed for 204 parts of phosphorus ( P) -doped tin oxide (Sn0 2 ) particles (phosphorus ( P) -containing tin oxide (Sn0 2 ) particles) disclosed in Example 1 of
  • Japanese Patent Application Laid-open No. H06-222600 (powder resistivity: 25 ⁇ -cm; amount of phosphorus ( P) doped to tin oxide (Sn0 2 ) (phosphorus ( P) dope level): 1% by mass) .
  • the metal oxide particles in the conductive layer coating fluid CI had an average particle diameter of 0.48 ⁇ .
  • a conductive layer coating fluid C2 was prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that 204 parts of the metal oxide particles, phosphorus ( P) -doped tin oxide (Sn0 2 ) coated titanium oxide (Ti0 2 ) particles, used therein in preparing the conductive layer coating fluid were changed for 204 parts of tungsten ( ) -doped tin
  • the metal oxide particles in the conductive layer coating fluid C2 had an average particle diameter of 0.65 ⁇ .
  • a conductive layer coating fluid C3 was prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that 204 parts of the metal oxide particles, phosphorus ( P) -doped tin oxide (SnC>2) coated titanium oxide (Ti0 2 ) particles, used therein in preparing the conductive layer coating fluid were changed for 204 parts of titanium oxide (Ti0 2 ) particles coated with oxygen deficient tin oxide (Sn0 2 ) as
  • particles in the conductive layer coating fluid C3 had an average particle diameter of 0.36 ⁇ .
  • a conductive layer coating fluid C4 was prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that 204 parts of the metal oxide particles, phosphorus ( P) -doped tin oxide (Sn0 2 ) coated titanium oxide (Ti0 2 ) particles, used therein in preparing the conductive layer coating fluid were changed for 204 parts of titanium oxide (Ti0 2 ) particles coated with antimony (Sb) -doped tin oxide (Sn0 2 ) ⁇ . as disclosed in Comparative Example 1 of Japanese Patent Application Laid-open No. Hll-007145 (titanium
  • Ti0 2 titanium oxide particles having coat layers of antimony oxide-containing tin oxide) (powder resistivity: 200 ⁇ -cm) .
  • the metal oxide particles in the conductive layer coating fluid C4 had an average particle diameter of 0.36 ⁇ .
  • a conductive layer coating fluid C5 was prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that 204 parts of the metal ⁇ oxide particles, phosphorus ( P) -doped tin oxide (Sn0 2 ) coated titanium oxide (Ti0 2 ) particles, used therein in preparing the conductive layer coating fluid were changed for .204 parts of barium sulfate (BaS0 4 )
  • a conductive layer coating fluid C6 was prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that 204 parts of the metal oxide particles, phosphorus ( P) -doped tin oxide (Sn0 2 ) coated titanium oxide (Ti0 2 ) particles, used therein in preparing the conductive layer coating fluid were changed for 240 parts of titanium oxide (Ti0 2 ) particles coated with oxygen deficient tin oxide (Sn0 2 ) as
  • the metal oxide particles in the conductive layer coating fluid C6 had an average particle diameter of 0.36 ⁇ .
  • a conductive layer coating fluid C7 was prepared in the same manner as Preparation Example of Conductive Layer Coating Fluid 1 except that 204 parts of the metal oxide particles, phosphorus ( P) -doped tin oxide (Sn0 2 ) coated titanium oxide (Ti0 2 ) particles, used therein in preparing the conductive layer coating fluid were changed for 204 parts of phosphorus ( P) -doped .
  • tin oxide (SnC>2) coated barium sulfate (BaS0 4 ) particles (powder resistivity: 40 ⁇ -cm; coverage of tin oxide: •35% by mass; amount of phosphorus ( P) doped to tin oxide (Sn0 2 ) (phosphorus (P) dope level): 3% by mass).
  • the metal oxide particles in the conductive layer coating fluid C7 had an average particle diameter of 0.40 ⁇ .
  • the conductive layer coating fluid 1 was dip-coated on the support in a 23°C/60%RH environment, and then the wet coating formed was dried and heat-cured at 140 °C for 30 minutes to form a conductive layer with a layer thickness of 30 ⁇ .
  • the volume resistivity of the conductive layer was measured by the method described previously, to find that it was 2.1*10 9 Q'cm.
  • polycarbonate resin (trade name: Z400; available from Mitsubishi Engineering-Plastics
  • This charge transport layer coating fluid was dip- coated on the charge generation layer, and then the wet coating formed was dried at 110°C for 30 minutes to form a charge transport layer with a layer thickness of 12 ⁇ .
  • an electrophotographic photosensitive member 1 was produced the charge transport layer of which was a surface layer.
  • the dielectric loss tan5 at frequency ⁇ . ⁇ ⁇ ⁇ 3 Hz, of the electrophotographic photosensitive member 1 was measured by the method described previously, to find that it was 7 ⁇ 10 ⁇ 3 .
  • Electrophotographic photosensitive members 2 to 20 and CI to C7 the charge transport layers of which were surface layers were produced in the same manner as Production Example of Electrophotographic
  • electrophotographic photosensitive member was changed for the conductive layer coating fluids 2 to 20 and CI to C7, respectively.
  • the dielectric loss tan5 at frequency ⁇ . ⁇ ⁇ ⁇ 3 Hz, of the electrophotographic photosensitive members 2 to 20 and CI to C7 each was measured like the electrophotographic photosensitive member 1 by the method described previously.
  • the volume resistivity of the conductive layer of the electrophotographic photosensitive members 2 to 20 and CI to C7 each was measured like the electrophotographic photosensitive member 1 by the method described previously. Results obtained thereon are shown in Table 2.
  • charge transport layer of which was a surface layer was produced in the same manner as Production Example of Electrophotographic Photosensitive Member 1 except that 10 parts of the charge-generating material,
  • hydroxygallium phthalocyanine crystals with a crystal form having intense peaks at 7.5°, 9.9°, 16.3°, 18.6°, 25.1° and 28.3° of the Bragg' s angle 2 ⁇ 0.2° in CuKa characteristic X-ray diffraction was changed for 10 parts of oxytitanium phthalocyanine crystals with a crystal form having intense peaks at 9.0°, 14.2°, 17.9°, 23.9° and 27.1° of the Bragg' s angle 2 ⁇ 0.2° in CuKa characteristic X-ray diffraction.
  • electrophotographic photosensitive member 21 and the volume resistivity of its conductive layer were
  • An electrophotographic photosensitive member 22 was
  • the dielectric loss tan5 at frequency ⁇ . ⁇ ⁇ ⁇ 3 Hz, of the electrophotographic photosensitive member 22 and the volume resistivity of its conductive layer were measured like the electrophotographic photosensitive member 1 by the methods described previously. Results obtained thereon are shown in Table 2.
  • Electrophotographic photosensitive members 1 to 22, and CI to C7 were each set in a laser beam printer (trade name: HP LASERJET P1505) manufactured by
  • the image evaluation was made on charging lines and on dots (black dots) and/or fog.
  • the evaluation on charging lines was made by using the one-dot keima

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Electrophotography Configuration And Component (AREA)
  • Electrostatic Charge, Transfer And Separation In Electrography (AREA)

Abstract

L'invention porte sur un élément photosensible électrophotographique qui ne peut pas provoquer facilement de chargement de lignes même dans l'endroit où se trouve un élément photosensible électrophotographique utilisant comme couche conductrice, une couche contenant des particules d'oxyde métallique. L'invention porte également sur une cartouche de traitement et sur un appareil électrophotographique qui ont un tel élément photosensible électrophotographique. L'élément photosensible électrophotographique a une couche conductrice qui contient des particules d'oxyde de titane revêtues d'oxyde d'étain dopé avec du phosphore ou du tungstène.
PCT/JP2010/065569 2009-09-04 2010-09-03 Élément photosensible électrophotographique, cartouche de traitement et appareil électrophotographique WO2011027911A1 (fr)

Priority Applications (7)

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RU2012112931/28A RU2507554C2 (ru) 2009-09-04 2010-09-03 Электрофотографический фоточувствительный элемент, технологический картридж и электрофотографическое устройство
KR1020127007842A KR101400650B1 (ko) 2009-09-04 2010-09-03 전자 사진 감광체, 프로세스 카트리지 및 전자 사진 장치
CN2010800389861A CN102483592B (zh) 2009-09-04 2010-09-03 电子照相感光构件、处理盒和电子照相设备
US13/384,852 US9256145B2 (en) 2009-09-04 2010-09-03 Electrophotographic photosensitive member, process cartridge, and electrophotographic apparatus
EP10813856.1A EP2443518B1 (fr) 2009-09-04 2010-09-03 Élément photosensible électrophotographique, cartouche de traitement et appareil électrophotographique
BR112012004861A BR112012004861A2 (pt) 2009-09-04 2010-09-03 membro fotossensível eletrofotográfico, cartucho de processo , e aparelho eletrofotográfico
US14/095,955 US10073362B2 (en) 2009-09-04 2013-12-03 Electrophotographic photosensitive member, process cartridge, and electrophotographic apparatus

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JP2009204522 2009-09-04
JP2009-204522 2009-09-04
JP2010-134306 2010-06-11
JP2010134306 2010-06-11
JP2010-196408 2010-09-02
JP2010196408A JP4743921B1 (ja) 2009-09-04 2010-09-02 電子写真感光体、プロセスカートリッジおよび電子写真装置

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US20120114375A1 (en) 2012-05-10
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US9256145B2 (en) 2016-02-09
CN102483592B (zh) 2013-08-28
EP3023840B8 (fr) 2018-03-21
RU2507554C2 (ru) 2014-02-20
US10073362B2 (en) 2018-09-11
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US20140093277A1 (en) 2014-04-03
EP3023840B1 (fr) 2018-02-14

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